EXPERIMENT NO.

Aim: - To see the grain structure of a mild steel specimen and compare its
structure with the displaced grain structure.

Objectives: (a) To Learn the preparation of specimen for microscopic observation.

(b) To understand what Microscopy is, and how it can be used to observe
microstructure of metals.

Apparatus : - (i) Metallurgical Microscope

(ii) Sample cutting equipment: Hack saw
(iii) Grinder
(iii) Specimen/Sample Mounting Hydraulic Press
(iv) Double disc polishing machine

Theory:-

Classification of Steel: The steels are classified by various methods and each method
is based on definite criteria as follows,
i) Amount of carbon
a) Low carbon steels (0.008 - 0.3%C)
b) Medium carbon steels (0.30 - 0.60%C)
c) High carbon steels (0.60 - 2.00%C)
ii) Amount of alloying elements and carbon
iii) Amount of de-oxidation
iv) Method of manufacture v) Form and use.

Grain: Many materials are formed of an aggregate of variously oriented crystals or

grains. Grains may be coarse or fine.
Grain boundary: A grain boundary (GB) is the interface between two grains, or
crystallites, in a polycrystalline material. Grain boundaries are defects in the crystal
structure, and tend to decrease the electrical and thermal conductivity of the material.
A grain boundary is a general planar defect that separates regions of different
crystalline orientation (such as grains) within a polycrystalline solid. Grain boundaries
are usually the result of uneven growth when the solid is crystallizing. Grain sizes vary
from 1 µm to 1 mm.

Polishing of small metallic specimen or of a specimen in the form of thin foil is difficult.
For convenience in handling during operation they are required to be attached to be
mounted on suitable plastic mold. This also helps in edge retention daring polishing.
The plastic mould is obtained from Bakelite powder by heating and pressure application.

This machine is used for mounting the specimen in a Bakelite powder & also to
handle properly the specimen during polishing. The unit is of a rugged construction and
is activated by a hydraulic press, capacity 5 tones. The unit is supplied with pressure
gauge to read the pressure being applied with mounting. The press is supplied with
mould heater with regulator & a timer. As a standard outfit, 25 mm diameter mold
assembly is supplied along with the machine. The mold is heat treated & internally
grounded alloy steel. This machine will also help to reduce the recurring cost of
consumable drastically unlike using cold setting compound. Other things required in the
process are as follows: Specimen beveller: Specimen beveller provides a simple and
positive method for ensuring that the metal surface is exactly perpendicular to the
optical axis of the microscope. The pressure on the plunger renders the upper polished
surface parallel to the under surface of the microscope slide on which it is mounted with
a plastic material. Metallographic linier polishing machine: This machine is used for
rough grinding of the mounted specimen. Generally, belt of number 80 to 100 are used.
Emery papers: Emery papers are used to do rough polishing of the specimen. These
papers have different grades according to grain size holding no: 100, 240, 320, and
400.

Particular features of interest are

(1) Grain size (II) phases present (III) Chemical homogeneity (IV) distribution of
phases (V) Elongated structures formed by plastic deformation

Procedure: - The preparation of metallic or other materials for microscopic examination

and micro structural characterization is in principal very simple. There are four basic
processes that you will need to become familiar with:
1. Sample cutting and sectioning,
2. Surface grinding and Lapping
3. Metallographic mounting
4.Surface polishing on double disc polishing machine
1 Sectioning
Sectioning means removal of convenient size specimen from large sample with minimal
damage to microstructure with the help of abrasive cut off machine. Abrasive cutting
wheel/saw is attached to cutting machine and for work piece holding proper vice is
provided on machine. The primary concern in this process is to minimize the heating of
the sample due to the cutting. For this reason, the cut-off saws that is equipped with
either water-cooling systems.

The goal of the surface polishing is to end up with a planar cross section of sample free
from scratches or disturbed metal introduced by the cutting and sectioning. This process
is a step-wise process that can be broken into three loosely separate parts: Grinding
and lapping, coarse polishing, and final polishing.
(2) Rough polishing (Grinding and Lapping): The first step in preparing your sample is to
ensure that you have a flat surface to begin with. A water-cooled abrasive grinder is available to
form a flat initial surface from which to begin. After getting a flat sample on the belt grinder,
WASH sample thoroughly. The hand lapping station has four graded abrasive papers to produce
a sequentially finer surface finish. Be sure the water is turned on and flowing uniformly over the
abrasives. Start with the coarsest grit (Sand paper/emery papers) (100) and, using a firm and
uniform pressure, slowly move the specimen forward and back across the abrasive. This will
produce parallel scratches of uniform size. Continue this step until the entire surface of your
sample is flat and contains only scratches of the size of 240 grit abrasive. When the sample is flat
and the only scratches remaining are those due to the 240 grit abrasive, WASH your sample and
your hands thoroughly, and move to the 400 grit abrasive

4 Mounting

The following process is used to encapsulate your specimen in Bakelite:

1) Place sample face down on the small piston inside the press, and lower the piston
into the cylinder by opening slightly the valve on the front of the press.
2) Approximately three tablespoons of Bakelite is poured over the sample, and the top
of the press gently screwed into place. DO NOT TIGHTEN THE TOP OF THE PRESS.
It is only necessary to engage all of the screw threads; you do not have to tightly secure
the top.
3) The cylindrical heater is plugged in and turned on (the red light should turn on). Place
the heater around the mold. The heater is thermostatically controlled and will heat the
mold to about 80 °C. Close the valve, and pump up the cylinder using the hand lever.
Now we press upon the piston by oscillating the jack handle in pumping action so that
the powder is compressed. A high pressure up to 1.5 to 2 MPa is required for it, which
can be read from the pressure gauge mounted on mounting pressure. As the Bakelite
heats, it will begin to flow to fill the void spaces, and the pressure will drop. Maintain the
constant.
4) Begin timing for 5-7 minutes to fully cure the Bakelite. Maintain the pressure during
the entire heating and cooling cycle.
5) At the end of the heating cycle, remove the heater and place the cooling collar on the
mold for an additional 6-8 minutes.
6) Crack the valve to release the pressure, and unscrew the top of the mold. When the
mold top is fully unscrewed (it may not come out due to adhesion with the Bakelite),
close the valve and slowly pump up the cylinder to push the sample fully out of the
press. Mark the sample on the back.
7) Clean any residual Bakelite off of the mold surfaces.

4 Sample Surface Polishing on double disc polishing machine

(i) Coarse polishing on double disc polishing machine

Before proceeding to the first polishing wheel (right most wheel), wash sample with water.
1) First, apply a small amount of water to the wheel, turn on the motor, and gently clean off the
wheel with your fingers.
2) Apply a small amount of abrasive slurry (polishing alumina) to the wheel. This wheel uses an
A1203 abrasive in a water suspension. The abrasive particles are 5 micrometers in diameter.
3) Carefully place your sample on the wheel while gripping it tightly. Slowly move the sample in
a circular motion against the rotation of the wheel. Use a moderate and even pressure. It is
important to ensure that you keep the sample flat on the wheel so that the final surface will be
completely planar.
4) After several minutes on the wheel, hold the sample in one place for a moment. This will
provide lots of parallel scratches that you can use to determine if you have removed the damage
from the grinding steps.
5) Examine the sample under the microscope to determine if all the scratches are the same size.

(ii) Final Polishing on double disc polishing machine

1) Repeat steps 1-5 above on the left polishing wheel. Carefully place your sample on the
wheel while gripping it tightly. This wheel uses buffing cloth abrasive. At this point, the
sample will be very smooth to the eye and even the oils and dirt on your fingers will
scratch it with larger scratches than the abrasive. DO NOT TOUCH THE SAMPLE
SURFACE FROM THIS POINT ON.
2) Etching: The last step in the process is to etch the sample to bring out the
microstructure. Grains cannot be seen without etching. Cracks, pores and defects are
observed without etching. The etching agent used is the solution of 95% distilled water,
2.5% nitric acid, 1.5% HCL and 1% fluoric acid.
3) Use a cotton swab and a petri dish for the etching. Gently swab the surface of your
sample with the etchant. Roughly spreading the etchant will scratch your surface. Let
the etchant stand for15 seconds or so and rinse the sample with water to stop the
etching. After last polishing stage the sample looks mirror like.
4) Examine specimen under the microscope.

5. OBSERVATION:
6. RESULT: The specimen is polished and can be used for watching the grain structure

7. PRECAUTIONS:
There are several general instructions to keep in mind during this part of the process.
1) CLEANLINESS!!! Keep the room and the work areas clean, especially the polishing
area. Each step in the polishing process uses a finer grade of abrasive, so good results
require that both your sample and your hands are free from abrasive at each stage
before proceeding to the next stage of the process. Turn the power off and cover the
wheels when you are through. Clean up any spilled water and wipe up the countertop.
2) Throw away the leftover etchants into the sink with a liberal amount of water. Swabs
should be rinsed and thrown into the trash bin IMMEDIATELY AFTER USE. Wash your
containers with water, rinse in methanol, and place them on the shelf above the sink.
3) Use goggles and gloves while handling chemicals. Contact the T.A. or the Instructor
in the case of an acid spill, or if new etchants are needed. Be extra careful when using
hydrofluoric acids.
4) Do not eat or drink anything while working in the lab. Wash your hands thoroughly
with soap before leaving the lab.